A kind of titanium silicon molecular sieve and its synthetic method and application and a kind of method of cyclic ketone oxidation

Abstract

The invention belongs to the field of titanium silicon molecular sieve, and more specifically provides a titanium silicon molecular sieve, and a synthetic method and applications thereof. The titaniumsilicon molecular sieve is composed of crystal particles with a particle size ranging from 5 to 200nm via aggregation; the particle size of the titanium silicon molecular sieve ranges from 0.3 to 5<mu>m; the I960 / I550 value ranges from 0.7 to 0.85. The invention also provides a cyclic ketone oxidation method. The cyclic ketone oxidation method comprises a step of contact of cyclic ketone, and anoxidizing agent with a catalyst. The catalyst contains the titanium silicon molecular sieve. The crystal of the titanium silicon molecular sieve is high in I960 / I550 value, and is large in effective framework ti content. When the titanium silicon molecular sieve is used in oxidation reaction, the catalytic oxidation activity, and the reaction product selectivity are increased obviously, and excellent catalytic stability is achieved. The titanium silicon molecular sieve is capable of realizing aggregation of small crystal particles in crystallization growth process instead of simple physical aggregation of the small crystal particles, and micron order is achieved.

Description

Technical field [0001] The invention relates to a titanium-silicon molecular sieve, a synthesis method and application thereof, and a method for oxidizing cyclic ketones. Background technique [0002] Titanium silicate molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. Among them, the titanium silicalite TS-1 not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 zeolite. Using titanium silicon molecular sieve as a catalyst can catalyze various types of organic oxidation reactions, such as epoxidation of alkenes, partial oxidation of alkanes, oxidation of alcohols, hydroxylation of phenols, and ammoxidation of cyclic ketones. As a catalyst for selective oxidation of organics, titanium-silica molecular sieve is considered a milestone in the field of molecular sieve catalysis. [0003] However, according to classic methods such as the method in US4410501, the particle s...

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Problems solved by technology

Therefore, follow-up research is devoted to the development of technologies for increasing the particle size of molecular sieves. For example, US5500199, US6106803 and US6524984, etc. use inorganic binders to gather small particle molecular sieves and then spray dry and granulate them to make the catalyst particles larger. The center is covered by the binder and the active components are diluted, resulting in insufficient reactivity and other problems

[0004] CN101696019B relates to a large block TS-1 molecular sieve with high catalytic activity and its synthesis method. The large block TS-1 molecular sieve has an MFI structure and is formed by stacking nanometer-level TS-1 grains, and the block size is larger. 20-100μm, the mesopore volume is 0.55cm 3 / g; with ethyl orthosilicate as silicon source, n-butyl titanate as titanium source, tetrapropylammonium hydroxide as template, water and isopropanol as solvent, H 2 o 2 It is synthesized by hydrothermal crystallization of inorganic additives, and the process is complicated

Although the obtained molecular sieve has high activity, the grain size is less than 1 μm

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